The emphasis of the proposed work is the synthesis and characterization of boron containing biomolecules. The importance of the research proposed stems from the fact that the molecules prepared could be used in boron neutron capture therapy (BNCT). This technique, although known for over 35 years, it is only recently gaining acceptance as an alternative method for the treatment of cancer, such as brain tumors or gliomas multiforme. There is a need for the preparation of more selective reagents for use in this technique, since the blood to tumor ration is still relatively low. Targeting molecules, such as amino acids, peptides, hormones and other regulatory molecules as components of the boronated unit, should enhance the selectivity of these compounds and result in a more efficient treatment using BNCT. Therefore, the main specific aim of the proposed work is the study of synthetic pathways leading to the preparation of this type of compounds. The implications of the biomedical field in cancer research can be staggering if the proposed results in the preparation of these types of compounds. The use of BNCT, in addition to other more traditional chemotherapeutical techniques can result in advancement of this approach to other types of cancer, besides brain tumors and gliomas. The synthetic techniques that will be employed to achieve the preparation of these compounds will be developed in the principal investigator's research laboratory and will be based, on some cases, on adaptations of known synthetic procedures use in boron hydride chemistry. Characterization of the prepared compounds will be achieved by using nuclear magnetic resonance (NMR) spectroscopy, Infrared spectroscopy, elemental analysis, mass spectrometry and when possible, single crystal X-ray crystallography of the synthesized compounds. The knowledge gained in the chemistry of these compounds will help advance the understanding of reaction conditions necessary for the preparation of these family of compounds and can result in the broad applicability of BNCT as an alternative or complimentary method in cancer treatment.